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C. Extraction<br />

( I) Place I OO-ml sample in 250-ml acid-washed separatory funnel. Adjust with buffer to pH 8.0 :!::0.5<br />

and add 2 ml of8-hydroxyquinoline solution.<br />

(2) Extract with 3 ml MIBK, shaking thoroughly. Collect extract (top) layer in very clean glassstoppered<br />

(or teflon) tubes for analysis.<br />

D. Analysis<br />

For the very low concentrations likely to be found , it will be necessary to inject MIBK-chelated metal<br />

into the flameless attachment of the atomic absorption spectrometer. Check manufacturer's handbook for<br />

complete details.<br />

6.4 Cadmium (Atomic Absorption)<br />

I. Concentrations<br />

Average river water = « I 0 /Lg / /<br />

Sea water = 0.0 1-0.1 I /Lg / /<br />

The dissolved sediment as prepared in Section 6.2 is analyzed by flame atomic absorption with the<br />

following opera ting parameters:<br />

A. Detection Limits<br />

Flame: 0.0 I mg/ / (solution) ( = 10 mg/ kg in sediment)<br />

B. Working Range<br />

Linear response of the spectrometer can be expected up to 2 mg/ / (solu tion) ( = 2 g/ kg of sediment).<br />

C. Interferences<br />

No serious chemical interferences.<br />

D. Instrument Parameters<br />

Wavelength: 228.8 nm<br />

Fuel: air/ acetylene<br />

Check manufacturer's handbook<br />

Flame: oxidizing (lean, blue)<br />

II. Solvent Extraction<br />

This method is necessary for the low concentrations found in seawater.<br />

A. Detection Limits<br />

Flameless: 0.00002 mg/ / (solution)<br />

B. Reagents<br />

( I) Chelating reagent: ammonium pyrrolidinedithiocarbamate (APDC) or sodium diethyldithiocarbamate<br />

(DEDC). Prepare a 5% solution with deionized-distilled water. A less concentrated solution ( 1-<br />

2%) may be found satisfactory for many situations. Extract at least twice with methyl isobutyl ketone<br />

(MIBK).<br />

(2) Methyl isobutyl ketone (MIBK) (distill to purify in all glass still).<br />

C. Extraction<br />

32

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